Captiva EMR-Lipid过滤柱净化结合液相色谱串联质谱法测定海产品中9种羟基多溴联苯醚

Determination of nine hydroxylated polybrominated diphenyl ethers in seafood by Captiva EMR-Lipid-filtration column purification combined with liquid chromatography tandem mass spectrometry

目的采用Captiva EMR-Lipid过滤柱净化处理技术简化样品前处理过程,结合液相色谱仪-串联质谱分析技术,确定特征离子对,优化液相及质谱参数,建立海产品中9种羟基多溴联苯醚(OH-BDEs)的测定方法。方法样品用乙腈超声萃取、Captiva EMR-Lipid过滤柱净化除脂,氮吹浓缩后采用液相色谱串联质谱(LC/MS/MS)电喷雾离子源(ESI)正离子模式测定,以多反应离子监测(MRM)模式扫描,保留时间及特征离子对定性,外标法定量。结果4′-OH-BDE-17、2′-OH-BDE-28、5-OH-BDE-47、6-OH-BDE-47、2′-OH-BDE-68、4-OH-BDE-42、6-OH-BDE-85、5′-OH-BDE-99、6′-OH-BDE-99等9种羟基多溴联苯醚在1 ng/ml~100 ng/ml内均呈现出良好线性关系,相关系数(r^(2))为0.9892~0.9973,检出限为0.01 ng/g~0.06 ng/g,不同基质3个水平的回收率为72.3%~109.1%,相对标准偏差(RSD)为5.2%~19.4%。结论本方法操作简单、准确快速、灵敏度高、精密度高,满足海产品中9种OH-BDEs的测定要求。

Objective In order to determine characteristic ion pairs and optimize liquid and mass spectrometry parameters,we used the technology of Captiva EMR-Lipid filtration column purification to simplify the pretreatment procedure,combined with liquid chromatograph-tandem mass spectrometry.Finally,a determination method for 9 hydroxylated polybrominated diphenyl ethers(OH-BDEs)in seafood was established.Methods The samples were extracted with acetonitrile by ultrasonic extraction and purified by Captiva EMR-Lipid filtration column.After nitrogen blowing and concentration,the samples were determined by liquid chromatography tandem mass spectrometry(LC/MS/MS)in electrospray ion source(ESI)positive ion mode.The samples were scanned by multiple reaction ion monitoring(MRM)mode.The retention time and characteristic ion pair were qualified and quantified by external standard method.Results Nine hydroxyl polybrominated diphenyl ethers such as 4′-OH-BDE-17,2′-OH-BDE-28,5-OH-BDE-47,6-OH-BDE-47,2′-OH-BDE-68,4-OH-BDE-42,6-OH-BDE-85,5′-OH-BDE-99,6′-OH-BDE-99 showed good linearity in the range of 1 ng/ml-100 ng/ml with correlation coefficients(r^(2))of 0.9892-0.9973.The detection limits of hydroxyl polybrominated diphenyl ethers were0.01 ng/g-0.06 ng/g.The recoveries at three levels of different matrices were 72.3%-109.1%,and the relative standard deviations(RSDs)were 5.2%-19.4%.Conclusion The method is simple,accurate and rapid with high sensitivity and precision,which can meet the determination requirements of 9 kinds of OH-BDEs in seafood.